CN110441115B - Preparation method of multilayer film X-ray zone plate - Google Patents
Preparation method of multilayer film X-ray zone plate Download PDFInfo
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- CN110441115B CN110441115B CN201910857821.XA CN201910857821A CN110441115B CN 110441115 B CN110441115 B CN 110441115B CN 201910857821 A CN201910857821 A CN 201910857821A CN 110441115 B CN110441115 B CN 110441115B
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a preparation method of a multilayer film X-ray zone plate, which comprises the following steps: vertically fixing the filamentous sample on the side surface of the sample holder; only cutting the multilayer film of the filiform sample by FIB cutting, and vertically cutting the visible part of the multilayer film into a specified thickness from top to bottom; soaking the cut part of the sample with liquid glue; turning the uncut multilayer film part upwards by rotation, fixing a copper foil at the cut position by using liquid glue in a contact manner, and completely cutting off the multilayer film at two sides of the remained multilayer film and the central wire by using FIB (focused ion beam); transferring the zone plate cut in the step by using a manipulator; fixing the zone plate at a specific position of the carrier net by using an FIB deposition technology; the cutting mechanical arm is used for polishing the zone plate to obtain the zone plate to be prepared; the invention can realize the preparation of the ultrathin zone plate, can protect the multilayer film of the zone plate, and strengthens the self-supporting capability of the ultrathin zone plate because of the protection of the liquid glue.
Description
Technical Field
The invention relates to the technical field of preparation of X-ray zone plates, in particular to a preparation method of a multilayer film X-ray zone plate.
Background
The X-ray wavelength is between 0.01 and 10nm, and the X-ray microscopic technology can be used for nondestructive detection and three-dimensional microscopic imaging of substances. The zone plate is a core element of an X-ray microscopic imaging technology, and when the zone plate is prepared by using a slice method at present, a hard X-ray zone plate with a large height-width ratio can be easily prepared, but if a soft X-ray zone plate with a smaller thickness is prepared by using the slice method, the problem is that a multilayer film is easily damaged. Also, if there is a gap between the multilayer film and the central filament, the self-supporting ability becomes problematic.
Therefore, when an ultrathin zone plate is manufactured, how to ensure a multilayer film without damaging the zone plate and how to ensure the self-supporting capability of the ultrathin zone plate are technical problems to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a multilayer film X-ray zone plate, which aims to solve the problems in the prior art, realize the preparation of an ultrathin zone plate, protect the multilayer film of the zone plate and strengthen the self-supporting capability of the ultrathin zone plate due to the protection of liquid glue.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation method of a multilayer film X-ray zone plate, which comprises the following steps:
(1) vertically fixing the filamentous sample on the side surface of the sample holder;
(2) only cutting the multilayer film of the filiform sample by FIB cutting, and vertically cutting the visible part of the multilayer film into a specified thickness from top to bottom;
(3) soaking the cut part of the sample with liquid glue;
(4) turning the uncut multilayer film part in the step 2 upwards by rotation, fixing a copper foil at the cut position in the step 2 by using liquid glue in a contact manner, and completely cutting off the multilayer films at two sides of the multilayer film reserved in the step 2 and the central wire by using FIB;
(5) carrying out the zone plate transfer cut in the step by using a manipulator;
(6) fixing the zone plate at a specific position of the carrier net by using an FIB deposition technology;
(7) and the cutting mechanical arm is used for polishing the zone plate to obtain the zone plate required to be prepared.
Preferably, the sample support is of a cube structure, the filamentous sample is adhered to the side face of the sample support through liquid glue, and the fixed filamentous sample is horizontally suspended.
Preferably, the sample is rotated 180 ° off by mechanical rotation, with the uncut multilayer film portion in step 2 facing upwards.
Preferably, the manipulator is severed using FIB.
Preferably, the zone plate is polished using FIB.
Compared with the prior art, the invention has the following beneficial technical effects:
the preparation method of the multilayer film X-ray zone plate can realize the preparation of the ultrathin zone plate, can protect the multilayer film of the zone plate, and can strengthen the self-supporting capability of the ultrathin zone plate because of the protection of the liquid glue.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic diagram of step 1 of a method of making a multilayer film X-ray zone plate according to the present invention;
FIG. 2 is a schematic view of step 2 of the method of making a multilayer film X-ray zone plate of the present invention;
FIG. 3 is a schematic diagram of step 4 of the method of making a multilayer film X-ray zone plate of the present invention;
FIG. 4 is a schematic view of step 6 of the method of making a multilayer film X-ray zone plate of the present invention;
in the figure: 1-filamentous sample, 2-sample holder, 3-central filament, 4-multilayer film, 5-copper foil, 6-zone plate and 7-grid.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a preparation method of a multilayer film X-ray zone plate, which aims to solve the problems in the prior art.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
The invention provides a preparation method of a multilayer film X-ray zone plate, which comprises the following steps:
(1) as shown in fig. 1, a filamentous sample 1 is vertically fixed on the side surface of a sample holder 2; the sample holder 2 is in a cube structure, the filamentous sample 1 is adhered to the side surface of the sample holder 2 through liquid glue, and the fixed filamentous sample 1 is horizontally suspended;
(2) only the multilayer film 4 of the filiform sample 1 is cut by FIB cutting, and the visible part of the multilayer film 4 is cut into a specified thickness vertically from top to bottom; as shown in fig. 2, a central cylindrical central filament 3 is surrounded by a multi-layer film 4 formed by laminating a plurality of films; the thickness of the multilayer film 4 remained after cutting is less than 1um, the distance remained on two sides is 20um, and the radian of the cut circle is 300 degrees;
(3) soaking the cut part of the sample with liquid glue; the liquid glue can wrap the cut multilayer film 4 part of the zone plate after being dried; in the invention, after the cut part of the sample is soaked by liquid glue, the multilayer films 4 wrapped outside the central wire 3 can be bonded, so that the multilayer films 4 can be bonded and can not be scattered, thus the self-supporting capability of the multilayer films is improved;
(4) as shown in fig. 3, the sample is rotated by 180 degrees through mechanical rotation, the uncut multilayer film part in the step 2 is upward, a copper foil 5 is fixed by contacting the cut position in the step 2 with liquid glue, and then the multilayer film at two sides of the multilayer film reserved in the step 2 and the central wire 3 are completely cut off by using FIB;
(5) transferring the zone plate 6 cut in the step by using a manipulator;
(6) as shown in fig. 4, FIB is used to deposit a fixed zone plate 6 at a specific position of the carrier net 7; the carrier net 7 can be understood as a clamp, and the carrier net 7 is fixed subsequently, so that the closer the zone plate 6 is to the center of the light through hole, the better;
(7) and the cutting mechanical arm is used for polishing the zone plate 6 to obtain the zone plate to be prepared.
The FIB and FIB deposition techniques of the present invention are specifically explained as follows:
FIB is a focused ion beam, which uses an electric lens to focus an ion beam into a very small size to bombard the surface of a material, thereby achieving the stripping, deposition (sputtering), implantation, cutting and modification of the material. With the development of nanotechnology, the nanoscale manufacturing industry is rapidly developed, nano processing is the core part of the nano manufacturing industry, a representative method of nano processing is focused ion beams, ion beams generated by an ion source are accelerated by an ion gun, and the focused ion beams act on the surface of a product to be cut, and mainly high-current ion beams strip surface atoms to finish the processing of micro-scale and nano-scale surfaces.
The principle and the implementation mode of the invention are explained by applying specific examples, and the description of the above examples is only used for helping understanding the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In summary, this summary should not be construed to limit the present invention.
Claims (5)
1. A preparation method of a multilayer film X-ray zone plate is characterized by comprising the following steps:
(1) vertically fixing a filamentous sample on the side surface of a sample support, adhering the filamentous sample to the side surface of the sample support through a liquid adhesive, horizontally suspending the fixed filamentous sample, wherein the filamentous sample comprises a central wire and a multilayer film wrapped on the outer side of the central wire, the central wire is cylindrical, and the periphery of the central wire is the multilayer film formed by overlapping layers of films;
(2) selecting two cutting positions on the filamentous sample along the axial direction by using FIB cutting, only cutting the multilayer film of the filamentous sample, vertically cutting the multilayer film at the top of the filamentous sample from top to bottom at the two cutting positions during cutting, wherein the multilayer film at the bottom of the filamentous sample after cutting is in an incomplete cutting state, the axial thickness of the multilayer film which is independently arranged between the two cutting positions after cutting at the top is less than 1 mu m, and gaps of 20 mu m are respectively cut at two sides of the independent multilayer film;
(3) soaking the sample cutting part with liquid glue, drying the liquid glue to wrap the multilayer film part of the cut zone plate, and after soaking the sample cutting part with the liquid glue, bonding the multilayer films wrapped on the outer side of the central wire, wherein the multilayer films are bonded, so that the self-supporting capacity of the multilayer films is improved;
(4) turning the uncut multilayer film part in the step 2 upwards by rotation, fixing a copper foil at the cut position in the step 2 by using liquid glue in a contact manner, and completely cutting the multilayer film which is not completely cut at the bottom of the filamentous sample in the step 2 and the central wire by using FIB;
(5) carrying out the zone plate transfer cut in the step by using a manipulator;
(6) fixing the zone plate at a specific position of the carrier net by using an FIB deposition technology;
(7) and the cutting mechanical arm is used for polishing the zone plate to obtain the zone plate required to be prepared.
2. A method of producing a multilayer film X-ray zone plate according to claim 1, characterized in that: the sample holder is of a cubic structure.
3. A method of producing a multilayer film X-ray zone plate according to claim 1, characterized in that: the sample holder was rotated 180 ° by mechanical rotation, with the uncut multilayer film portion in step 2 facing upwards.
4. A method of producing a multilayer film X-ray zone plate according to claim 1, characterized in that: the manipulator is cut using FIB.
5. A method of producing a multilayer film X-ray zone plate according to claim 1, characterized in that: the zone plate is polished using FIB.
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| CN201910857821.XA CN110441115B (en) | 2019-09-09 | 2019-09-09 | Preparation method of multilayer film X-ray zone plate |
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| CN201910857821.XA CN110441115B (en) | 2019-09-09 | 2019-09-09 | Preparation method of multilayer film X-ray zone plate |
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| CN110441115B true CN110441115B (en) | 2022-02-22 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6337302A (en) * | 1986-08-01 | 1988-02-18 | Sanyo Electric Co Ltd | Production of fresnel zone plate |
| CN1680504A (en) * | 2004-04-01 | 2005-10-12 | 国家淀粉及化学投资控股公司 | Dicing die bonding film |
| CN106167683A (en) * | 2015-05-18 | 2016-11-30 | 日东电工株式会社 | The one-piece type adhesive foil of adhesive foil, dicing tape, plural layers, the manufacture method of semiconductor device and semiconductor device |
| CN107833649A (en) * | 2017-10-16 | 2018-03-23 | 中国科学院电工研究所 | A kind of preparation method of X ray zone plate |
| CN110060793A (en) * | 2019-05-05 | 2019-07-26 | 中国科学院电工研究所 | A kind of preparation method of X-ray zone plate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104317160A (en) * | 2014-09-19 | 2015-01-28 | 京东方科技集团股份有限公司 | Mask, spacer formed by the mask and preparation method of spacer by using the mask |
| US10500825B2 (en) * | 2015-04-29 | 2019-12-10 | Wolverine Automotive Board Sales, Inc. | Extensible paper laminates and their uses |
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2019
- 2019-09-09 CN CN201910857821.XA patent/CN110441115B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6337302A (en) * | 1986-08-01 | 1988-02-18 | Sanyo Electric Co Ltd | Production of fresnel zone plate |
| CN1680504A (en) * | 2004-04-01 | 2005-10-12 | 国家淀粉及化学投资控股公司 | Dicing die bonding film |
| CN106167683A (en) * | 2015-05-18 | 2016-11-30 | 日东电工株式会社 | The one-piece type adhesive foil of adhesive foil, dicing tape, plural layers, the manufacture method of semiconductor device and semiconductor device |
| CN107833649A (en) * | 2017-10-16 | 2018-03-23 | 中国科学院电工研究所 | A kind of preparation method of X ray zone plate |
| CN110060793A (en) * | 2019-05-05 | 2019-07-26 | 中国科学院电工研究所 | A kind of preparation method of X-ray zone plate |
Non-Patent Citations (1)
| Title |
|---|
| 聚焦离子束切割法制备多层膜Ｘ射线波带片;姚广宇 等;《微纳电子技术》;20190430;第56卷(第4期);第314-318页 * |
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